반응 #41182

ord-3588cffdb1fd4428bec73a63ad14976a

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated to 40° C. in a preheated oil bath for 4 hours
  2. 2
    온도The reaction was then cooled to room temperature
  3. 3
    농축concentrated
  4. 4
    기타to remove the ethanol
  5. 5
    workup.ADDITIONTo the flask was added water (20 mL)
  6. 6
    추출the aqueous layer was extracted with diethyl ether (2×100 mL)
  7. 7
    건조dried over anhydrous Na2SO4
  8. 8
    여과filtered
  9. 9
    농축concentrated

실험 절차

To a solution of hydrazine monohydrate (36.0 mL, 0.750 mol) in ethanol (70 mL) at 0° C. in an ice-water bath was added 2-(2-bromoethoxy)-2-methylpropane (12.1 mL, 0.075 mol) drop-wise over 20 minutes. The reaction was then allowed to warm to room temperature and stir for 5 minutes and then heated to 40° C. in a preheated oil bath for 4 hours. The reaction was then cooled to room temperature and concentrated to remove the ethanol. To the flask was added water (20 mL) and the aqueous layer was extracted with diethyl ether (2×100 mL). The organic layers were combined and dried over anhydrous Na2SO4, filtered and concentrated to provide (2-tert-butoxyethyl)-hydrazine as a colorless oil (6.05 g, 61%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07728029B2uspto-grants-2010_06